CN107964213A - One kind load graphene nano level melamine bubble silk floss and preparation method thereof - Google Patents
One kind load graphene nano level melamine bubble silk floss and preparation method thereof Download PDFInfo
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- CN107964213A CN107964213A CN201711487679.1A CN201711487679A CN107964213A CN 107964213 A CN107964213 A CN 107964213A CN 201711487679 A CN201711487679 A CN 201711487679A CN 107964213 A CN107964213 A CN 107964213A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2361/00—Characterised by the use of condensation polymers of aldehydes or ketones; Derivatives of such polymers
- C08J2361/20—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C08J2361/26—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds
- C08J2361/28—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds with melamine
Abstract
The present invention relates to one kind load graphene nano level melamine bubble silk floss, including following parts by weight component raw material：1 15 parts of melamine, 25 90 parts of formalin, 18 parts of basic catalyst, 38 parts of modified graphene, 40 70 parts of acid regulator, 6 15 parts of surfactant, 12 28 parts of foaming agent, 5 15 parts of modifying agent；During its preparation method, first prepare melamine resin, then the graphene oxide being modified by graphene, the concentrated sulfuric acid, concentrated phosphoric acid, potassium permanganate and melamine resin are made after load graphene nano level melamine foam by ultrasonic emulsification, microwave foaming and are gone out formaldehyde by high temperature, obtain the load graphene nano level melamine foam of low formaldehyde；The present invention has the advantages that high mechanical strength, production efficiency are high, water imbibition is strong, environmental protection.
Description
Technical field
The invention belongs to polyvinyl formal foam technology field, and in particular to one kind load graphene nano level three
Poly cyanamid bubble silk floss and preparation method thereof.
Background technology
Melamine foam be Novel clean, sound insulation, insulation multifunctional material, be widely used in bullet train every
The fields such as sound, environment cleaning, insulation of equipment.The water imbibition for the melamine foam for being usually used in cleaning applications at present is poor,
When wiping object water stain at once, it is impossible to exhaust water stain, nor can effectively absorb the spot of body surface, lead
Cause the continuous cleaning effect of melamine bubble undesirable；And graphene oxide has good hydrophily, water can be effectively adsorbed
Stain, is good hydrophilic substance.Moreover, current melamine foam low production efficiency, when melamine resin emulsifies
Between it is long, scared efficiency is low, seriously affects the continuous production efficiency of melamine bubble, for enterprise's life ginseng, its economic benefit ratio
It is relatively low.
The content of the invention
It is high, hydrophilic that a kind of high mechanical strength, production efficiency are provided the purpose of the present invention is overcome the deficiencies in the prior art
Property strong, environmental protection load graphene nano level melamine bubble silk floss and preparation method thereof.
Technical scheme is as follows：
One kind load graphene nano level melamine bubble is continuous, including following parts by weight component raw material：1-15 parts of melamine,
25-90 parts of formalin, 1-8 parts of basic catalyst, 3-8 parts of modified graphene, 40-70 parts of acid regulator, surfactant
6-15 parts, 12-28 parts of foaming agent, 5-15 parts of modifying agent.
Preferably, the modified graphene is graphene oxide powder.
Preferably, the content of formaldehyde is 36%-40% in the formalin.
Preferably, the basic catalyst is at least one in diethanol amine, sodium hydroxide, calcium hydroxide, monoethanolamine
Kind.
Preferably, the acid regulator is at least one of hydrochloric acid, oxalic acid, aphthenic acids, acetic acid.
Preferably, the surfactant is lauryl sodium sulfate, sodium sulfate of polyethenoxy ether of fatty alcohol, dodecyl
At least one of ethyoxyl sulfobetaines, phosphate-based glycine betaine.
Further, the continuous preparation method of the load graphene nano level melamine bubble, comprises the following steps：
1）, prepare modified graphene；
2）, weigh melamine, formalin and basic catalyst in parts by weight and be added to heating stirring in reactor, add
Hot temperature is 55 DEG C -75 DEG C, and mixing time 30min-45min obtains melamine resin；
3）, complete step 2）Afterwards, temperature of reactor is down to 70 DEG C, modified graphene powder is added during stirring is continued
End, while apply ultrasonic wave ancillary vibration stirring 15min-30min and obtain emulsifying mixt；
4）, by step 3）Obtained emulsifying mixt adds progress microwave foamed solidification in microwave foaming machine and obtains load graphene
Nanoscale melamine foam.
Preferably, the step 4）The microwave frequency of middle application is 2450MHz.
Further, the step 1）Specific practice is as follows, measures a certain amount of concentrated sulfuric acid and concentrated phosphoric acid respectively, adds scale
Graphite, potassium permanganate, are warming up to 35 DEG C, after reacting 3 h, add distilled water, after the reaction was continued 30 min, the 10% of addition
H2O2, the reaction was continued 20min, filter, with 1 molL- 1Hydrochloric acid and distilled water wash repeatedly to neutrality after it is dry, obtain
Graphene oxide.
Further, the step 4 is completed）Afterwards, by 60 DEG C -80 of the continuous immersion of the load graphene nano level melamine bubble
DEG C hot water in 15min-45min, then at a temperature of 180 DEG C -300 DEG C toast 30min-90min remove formaldehyde.
Compared with prior art, the beneficial effects of the invention are as follows：
The present invention adds modified graphene in melamine resin, and wherein modified graphene uses graphene oxide, from
And the hydrophily of melamine foam is improved, effectively improve the soaking effect of melamine foam so that melamine foam has
There is good cleaning effect；Modified graphene, melamine are improved using the surfactant with emulsification, foaming, peptizaiton
Pulling force between amine and formaldehyde, emulsification rapidly and efficiently is carried out at a temperature of 70 DEG C using ultrasonic emulsification device, is then passed through
Microwave foaming machine carries out microwave foaming, and the moisture in foaming body and organic gas effectively are mentioned surface and are removed, is had
Effect improves the continuous production efficiency of bubble, and after ultrasonic emulsification and microwave foaming, it is continuous to effectively improve melamine resin bubble
Mechanical strength；It will finally steep after being toasted in the continuous hot water for immersing 60 DEG C -80 DEG C, formaldehyde unnecessary in de-bubble silk floss removed, so as to have
Effect improves the continuous environmental-protecting performance of bubble；In short, the present invention is strong, environmental protection excellent with high mechanical strength, production efficiency height, hydrophily
Point.
Embodiment
Below in conjunction with the embodiment of the present invention, the technical solution in the embodiment of the present invention is clearly and completely described,
Obviously, described embodiment is only part of the embodiment of the present invention, instead of all the embodiments.Based in the present invention
Embodiment, those of ordinary skill in the art's all other embodiments obtained without making creative work, all
Belong to the scope of protection of the invention.
Embodiment 1
One kind load graphene nano level melamine bubble is continuous, including following parts by weight component raw material：1 part of melamine, first
25 parts of aldehyde solution, 1 part of basic catalyst, 3 parts of modified graphene, 40 parts of acid regulator, 6 parts of surfactant, foaming agent 12
Part, 5 parts of modifying agent.
In the present embodiment, the modified graphene is graphene oxide powder；The content of formaldehyde is in the formalin
36%；The basic catalyst is diethanol amine；The acid regulator is hydrochloric acid；The surfactant is dodecyl sulphur
Sour sodium.
Further, the continuous preparation method of the load graphene nano level melamine bubble, comprises the following steps：
1）, prepare modified graphene；
2）, weigh melamine, formalin and basic catalyst in parts by weight and be added to heating stirring in reactor, add
Hot temperature is 55 DEG C, and mixing time 30min obtains melamine resin；
3）, complete step 2）Afterwards, temperature of reactor is down to 70 DEG C, modified graphene powder is added during stirring is continued
End, while apply ultrasonic wave ancillary vibration stirring 15min and obtain emulsifying mixt；
4）, by step 3）Obtained emulsifying mixt adds progress microwave foamed solidification in microwave foaming machine and obtains load graphene
Nanoscale melamine foam, wherein the microwave frequency applied is 2450MHz；
5）, by 15min in the continuous hot water for immersing 60 DEG C of load graphene nano level melamine bubble, then in 180 DEG C of temperature
The lower baking 90min of degree removes formaldehyde.
Wherein, the step 1）Specific practice is as follows, measures a certain amount of concentrated sulfuric acid and concentrated phosphoric acid respectively, adds scale stone
Ink, potassium permanganate, are warming up to 35 DEG C, after reacting 3 h, add distilled water, after the reaction was continued 30 min, the 10% of addition
H2O2, the reaction was continued 20min, filter, with 1 molL- 1Hydrochloric acid and distilled water wash repeatedly to neutrality after it is dry, obtain
Graphene oxide.
Embodiment 2
One kind load graphene nano level melamine bubble is continuous, including following parts by weight component raw material：15 parts of melamine, first
90 parts of aldehyde solution, 8 parts of basic catalyst, 8 parts of modified graphene, 70 parts of acid regulator, 15 parts of surfactant, foaming agent 28
Part, 15 parts of modifying agent.
In the present embodiment, the modified graphene is graphene oxide powder；The content of formaldehyde is in the formalin
40%；The basic catalyst is sodium hydroxide；The acid regulator is oxalic acid；The surfactant is fatty alcohol polyoxy
Ethene ether sodium sulfate.
Further, the continuous preparation method of the load graphene nano level melamine bubble, comprises the following steps：
1）, prepare modified graphene；
2）, weigh melamine, formalin and basic catalyst in parts by weight and be added to heating stirring in reactor, add
Hot temperature is 75 DEG C, and mixing time 45min obtains melamine resin；
3）, complete step 2）Afterwards, temperature of reactor is down to 70 DEG C, modified graphene powder is added during stirring is continued
End, while apply ultrasonic wave ancillary vibration stirring 30min and obtain emulsifying mixt；
4）, by step 3）Obtained emulsifying mixt adds progress microwave foamed solidification in microwave foaming machine and obtains load graphene
Nanoscale melamine foam, wherein the microwave frequency applied is 2450MHz；
5）, by 45min in the continuous hot water for immersing 80 DEG C of load graphene nano level melamine bubble, then in 300 DEG C of temperature
The lower baking 30min of degree removes formaldehyde.
Wherein, the step 1）Specific practice is as follows, measures a certain amount of concentrated sulfuric acid and concentrated phosphoric acid respectively, adds scale stone
Ink, potassium permanganate, are warming up to 35 DEG C, after reacting 3 h, add distilled water, after the reaction was continued 30 min, the 10% of addition
H2O2, the reaction was continued 20min, filter, with 1 molL- 1Hydrochloric acid and distilled water wash repeatedly to neutrality after it is dry, obtain
Graphene oxide.
Embodiment 3
One kind load graphene nano level melamine bubble is continuous, including following parts by weight component raw material：10 parts of melamine, first
30 parts of aldehyde solution, 5 parts of basic catalyst, 5 parts of modified graphene, 55 parts of acid regulator, 12 parts of surfactant, foaming agent 25
Part, 8 parts of modifying agent.
In the present embodiment, the modified graphene is graphene oxide powder；The content of formaldehyde is in the formalin
37%；The basic catalyst is calcium hydroxide；The acid regulator is aphthenic acids；The surfactant is dodecyl
Ethyoxyl sulfobetaines.
Further, the continuous preparation method of the load graphene nano level melamine bubble, comprises the following steps：
1）, prepare modified graphene；
2）, weigh melamine, formalin and basic catalyst in parts by weight and be added to heating stirring in reactor, add
Hot temperature is 60 DEG C, and mixing time 31min obtains melamine resin；
3）, complete step 2）Afterwards, temperature of reactor is down to 70 DEG C, modified graphene powder is added during stirring is continued
End, while apply ultrasonic wave ancillary vibration stirring 18min and obtain emulsifying mixt；
4）, by step 3）Obtained emulsifying mixt adds progress microwave foamed solidification in microwave foaming machine and obtains load graphene
Nanoscale melamine foam, wherein the microwave frequency applied is 2450MHz；
5）, by 20min in the continuous hot water for immersing 70 DEG C of load graphene nano level melamine bubble, then in 250 DEG C of temperature
The lower baking 60min of degree removes formaldehyde.
Wherein, the step 1）Specific practice is as follows, measures a certain amount of concentrated sulfuric acid and concentrated phosphoric acid respectively, adds scale stone
Ink, potassium permanganate, are warming up to 35 DEG C, after reacting 3 h, add distilled water, after the reaction was continued 30 min, the 10% of addition
H2O2, the reaction was continued 20min, filter, with 1 molL- 1Hydrochloric acid and distilled water wash repeatedly to neutrality after it is dry, obtain
Graphene oxide.
Embodiment 4
One kind load graphene nano level melamine bubble is continuous, including following parts by weight component raw material：5 parts of melamine, first
50 parts of aldehyde solution, 6 parts of basic catalyst, 4 parts of modified graphene, 45 parts of acid regulator, 10 parts of surfactant, foaming agent 23
Part, 6 parts of modifying agent.
In the present embodiment, the modified graphene is graphene oxide powder；The content of formaldehyde is in the formalin
39%；The basic catalyst is monoethanolamine；The acid regulator is acetic acid；The surfactant is phosphate-based sweet tea
Dish alkali.
Further, the continuous preparation method of the load graphene nano level melamine bubble, comprises the following steps：
1）, prepare modified graphene；
2）, weigh melamine, formalin and basic catalyst in parts by weight and be added to heating stirring in reactor, add
Hot temperature is 65 DEG C, and mixing time 33min obtains melamine resin；
3）, complete step 2）Afterwards, temperature of reactor is down to 70 DEG C, modified graphene powder is added during stirring is continued
End, while apply ultrasonic wave ancillary vibration stirring 20min and obtain emulsifying mixt；
4）, by step 3）Obtained emulsifying mixt adds progress microwave foamed solidification in microwave foaming machine and obtains load graphene
Nanoscale melamine foam, wherein the microwave frequency applied is 2450MHz；
5）, by 35min in the continuous hot water for immersing 75 DEG C of load graphene nano level melamine bubble, then in 200 DEG C of temperature
The lower baking 65min of degree removes formaldehyde.
Wherein, the step 1）Specific practice is as follows, measures a certain amount of concentrated sulfuric acid and concentrated phosphoric acid respectively, adds scale stone
Ink, potassium permanganate, are warming up to 35 DEG C, after reacting 3h, add distilled water, after the reaction was continued 30 min, 10% H2O2 of addition
, the reaction was continued 20min, filters, with 1 molL- 1Hydrochloric acid and distilled water wash repeatedly to neutrality after it is dry, aoxidized
Graphene.
Embodiment 5
One kind load graphene nano level melamine bubble is continuous, including following parts by weight component raw material：8 parts of melamine, first
60 parts of aldehyde solution, 3 parts of basic catalyst, 7 parts of modified graphene, 60 parts of acid regulator, 7 parts of surfactant, foaming agent 27
Part, 11 parts of modifying agent.
In the present embodiment, the modified graphene is graphene oxide powder；The content of formaldehyde is in the formalin
38%；The basic catalyst is calcium hydroxide；The acid regulator is hydrochloric acid；The surfactant is fatty alcohol polyoxy
Ethene ether sodium sulfate.
Further, the continuous preparation method of the load graphene nano level melamine bubble, comprises the following steps：
1）, prepare modified graphene；
2）, weigh melamine, formalin and basic catalyst in parts by weight and be added to heating stirring in reactor, add
Hot temperature is 70 DEG C, and mixing time 40min obtains melamine resin；
3）, complete step 2）Afterwards, temperature of reactor is down to 70 DEG C, modified graphene powder is added during stirring is continued
End, while apply ultrasonic wave ancillary vibration stirring 25min and obtain emulsifying mixt；
4）, by step 3）Obtained emulsifying mixt adds progress microwave foamed solidification in microwave foaming machine and obtains load graphene
Nanoscale melamine foam, wherein the microwave frequency applied is 2450MHz；
5）, by 32min in the continuous hot water for immersing 65 DEG C of load graphene nano level melamine bubble, then in 280 DEG C of temperature
The lower baking 40min of degree removes formaldehyde.
Wherein, the step 1）Specific practice is as follows, measures a certain amount of concentrated sulfuric acid and concentrated phosphoric acid respectively, adds scale stone
Ink, potassium permanganate, are warming up to 35 DEG C, after reacting 3 h, add distilled water, after the reaction was continued 30 min, the 10% of addition
H2O2, the reaction was continued 20min, filter, with 1 molL- 1Hydrochloric acid and distilled water wash repeatedly to neutrality after it is dry, obtain
Graphene oxide.
Embodiment 6
One kind load graphene nano level melamine bubble is continuous, including following parts by weight component raw material：6 parts of melamine, first
80 parts of aldehyde solution, 4 parts of basic catalyst, 6 parts of modified graphene, 65 parts of acid regulator, 9 parts of surfactant, foaming agent 18
Part, 16 parts of modifying agent.
In the present embodiment, the modified graphene is graphene oxide powder；The content of formaldehyde is in the formalin
36%；The basic catalyst is monoethanolamine；The acid regulator is aphthenic acids；The surfactant is dodecyl
Ethyoxyl sulfobetaines.
Further, the continuous preparation method of the load graphene nano level melamine bubble, comprises the following steps：
1）, prepare modified graphene；
2）, weigh melamine, formalin and basic catalyst in parts by weight and be added to heating stirring in reactor, add
Hot temperature is 63 DEG C, and mixing time 42min obtains melamine resin；
3）, complete step 2）Afterwards, temperature of reactor is down to 70 DEG C, modified graphene powder is added during stirring is continued
End, while apply ultrasonic wave ancillary vibration stirring 22min and obtain emulsifying mixt；
4）, by step 3）Obtained emulsifying mixt adds progress microwave foamed solidification in microwave foaming machine and obtains load graphene
Nanoscale melamine foam, wherein the microwave frequency applied is 2450MHz；
5）, by 40min in the continuous hot water for immersing 72 DEG C of load graphene nano level melamine bubble, then in 190 DEG C of temperature
The lower baking 80min of degree removes formaldehyde.
Wherein, the step 1）Specific practice is as follows, measures a certain amount of concentrated sulfuric acid and concentrated phosphoric acid respectively, adds scale stone
Ink, potassium permanganate, are warming up to 35 DEG C, after reacting 3 h, add distilled water, after the reaction was continued 30 min, the 10% of addition
H2O2, the reaction was continued 20min, filter, with 1 molL- 1Hydrochloric acid and distilled water wash repeatedly to neutrality after it is dry, obtain
Graphene oxide.
Although the present invention is described in detail with reference to the foregoing embodiments, for those skilled in the art,
It can still modify the technical solution described in foregoing embodiments, or which part technical characteristic is carried out etc.
With replacing, within the spirit and principles of the invention, any modification, equivalent replacement, improvement and so on, should be included in this
The protection domain of invention it.
Claims (10)
1. one kind load graphene nano level melamine bubble is continuous, it is characterised in that：Including following parts by weight component raw material：Three
1-15 parts of poly cyanamid, 25-90 parts of formalin, 1-8 parts of basic catalyst, 3-8 parts of modified graphene, acid regulator 40-70
Part, 6-15 parts of surfactant, 12-28 parts of foaming agent, 5-15 parts of modifying agent.
2. load graphene nano level melamine bubble is continuous as claimed in claim 1, it is characterised in that：The modified graphene
For graphene oxide powder.
3. load graphene nano level melamine bubble is continuous as claimed in claim 1, it is characterised in that：In the formalin
The content of formaldehyde is 36%-40%.
4. load graphene nano level melamine bubble is continuous as claimed in claim 1, it is characterised in that：The basic catalyst
For at least one of diethanol amine, sodium hydroxide, calcium hydroxide, monoethanolamine.
5. load graphene nano level melamine bubble is continuous as claimed in claim 1, it is characterised in that：The acid regulator
For at least one of hydrochloric acid, oxalic acid, aphthenic acids, acetic acid.
6. load graphene nano level melamine bubble is continuous as claimed in claim 1, it is characterised in that：The surfactant
For lauryl sodium sulfate, sodium sulfate of polyethenoxy ether of fatty alcohol, dodecyl ethyoxyl sulfobetaines, phosphate-based beet
At least one of alkali.
7. the continuous preparation method of load graphene nano level melamine bubble as claimed in claim 1, it is characterised in that including
Following steps：
1）, prepare modified graphene；
2）, weigh melamine, formalin and basic catalyst in parts by weight and be added to heating stirring in reactor, add
Hot temperature is 55 DEG C -75 DEG C, and mixing time 30min-45min obtains melamine resin；
3）, complete step 2）Afterwards, temperature of reactor is down to 70 DEG C, modified graphene powder is added during stirring is continued
End, while apply ultrasonic wave ancillary vibration stirring 15min-30min and obtain emulsifying mixt；
4）, by step 3）Obtained emulsifying mixt adds progress microwave foamed solidification in microwave foaming machine and obtains load graphene
Nanoscale melamine foam.
8. the continuous preparation method of load graphene nano level melamine bubble as claimed in claim 7, it is characterised in that：It is described
Step 4）The microwave frequency of middle application is 2450MHz.
9. the continuous preparation method of load graphene nano level melamine bubble as claimed in claim 7, it is characterised in that：It is described
Step 1）Specific practice is as follows, measures a certain amount of concentrated sulfuric acid and concentrated phosphoric acid respectively, adds crystalline flake graphite, potassium permanganate, heating
To 35 DEG C, after reacting 3 h, distilled water is added, after the reaction was continued 30 min, 10% H2O2 of addition, the reaction was continued
20min, filters, with 1 molL- 1Hydrochloric acid and distilled water wash repeatedly to neutrality after it is dry, obtain graphene oxide.
10. the continuous preparation method of load graphene nano level melamine bubble as claimed in claim 1, it is characterised in that：It is complete
Into the step 4）Afterwards, by 15min- in the continuous hot water for immersing 60 DEG C -80 DEG C of load graphene nano level melamine bubble
45min, then toasts 30min-90min at a temperature of 180 DEG C -300 DEG C and removes formaldehyde.
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